β-环糊精液相色谱柱测定黄瓜中灭菌唑对映体含量  

Enantioseparation and determination of triticonazole enantiomers in cucumber on β-cyclodextrin-based column by HPLC

作　　者：廖玉芹 曹志刚 雷学影 王惠 李来生 LIAO Yuqin;CAO Zhigang;LEI Xueying;WANG Hui;Li Laisheng(College of Chemistry,Nanchang University,Nanchang 330031,China)

机构地区：[1]南昌大学化学学院,江西南昌330031

出　　处：《南昌大学学报（理科版）》2017年第6期531-537,共7页Journal of Nanchang University(Natural Science)

基　　金：国家自然科学基金资助项目(21165012);江西省教育厅重点基金资助项目(GJJ150019);食品科学与技术国家重点实验室开放基金(SKLF-KF-201605)

摘　　要：手性农药对映体的差异性给食品安全带来了新问题。采用自制的邻苯二甲酰亚胺-β-环糊精手性固定相(PCDP),通过研究不同的流动相组成、柱温等条件对手性分离的影响,成功地拆分了四种常见的三唑类手性农药对映体,最大分离度达3.81。并选取灭菌唑为定量组分,黄瓜为果蔬样品,发展了一种测定黄瓜中灭菌唑对映体残留量的新方法。优化的流动相为甲醇-水(35:65,v/v),流速为0.5mL·min-1,柱温为293K(20℃),进样量为10μL,检测波长为260nm。实验结果表明,灭菌唑对映体的线性关系良好(r2=0.986 5),线性范围均为(1~50μg·mL-1)。灭菌唑第一个对映体的加标平均回收率为92.54%,RSD为1.15%;第二个对映体的加标平均回收率为93.16%,RSD为1.23%。黄瓜中两对映体的检出限小于20μg·kg-1。该方法操作简便,测定快速,结果准确,重现性好,自制的环糊精键合相成本较低,对果蔬中手性农药灭菌唑对映体残留量的检测有实用性。The difference of chiral pesticide enantiomers in biological activity has brought new chiral problems to food safety.In this paper,a home-made phthalimide-β-cyclodextrin chiral stationary phase(PCDP)was successfully used for enantioseparation of four common triazole chiral pesticides through the optimization of different mobile phase composition,column temperature and other conditions,where the maximum resolution was 3.81.Based on the above study,a new method was developed to determine the triticonazole enantiomers residues in cucumber onβ-cyclodextrin-based column was developed by HPLC.The optimized mobile phase was methanol-water(35:65,v/v),the flow rate was 0.5 mL·min-1,the column temperature was 293K(20℃),the injection volume was 10μL and the detection wavelength was 260 nm.The experimental results showed that the good linear relationship(r 2=0.986 5)with linear range(1~50μg·mL-1)was observed for both triticonazole enantiomers.The spiked average recovery of the first enantiomer of the triticonazole was 92.54%with a RSD of 1.15%.The average spiked recovery of the second enantiomer was 93.16%with a RSD of 1.23%.The detection limits of two enantiomers in cucumber were less than 20μg·kg-1.The method had the advantages of simple and convenient operation,rapid determination,accurate result and good reproducibility,and it was suitable for determining the residues of triticonazole enantiomerics in fruits and vegetables.

关 键 词：液相色谱法 β-环糊精固定相 分离与测定 灭菌唑对映体 黄瓜 

分 类 号：O658[理学—分析化学]